UPLC-MS/MS法检测抗癫痫中成药中非法添加苯巴比妥和卡马西平

目的：建立抗癫痫中成药中非法添加苯巴比妥和卡马西平的UPLC-MS/MS检测方法。方法：采用Waters ACQUITY UPLC/Quattro Premier液质联用仪，以BEH-C₁₈（100 mm×2.1 mm，1.7 μm）色谱柱分离，0.02 mol·L^-1醋酸铵水溶液-乙腈（1：1）为流动相，质谱检测器采用多反应监测（MRM）模式进行定性定量检测;供试样品的处理，采用以甲醇为溶剂的超声提取方法。结果：苯巴比妥和卡马西平的保留时间分别为1.1 min和1.3 min，检测限分别为2.2 μg·mL^-1和0.10 μg·mL^-1，定量限分别为7.5 μg·mL^-1和0.35 μg·mL^-1，标准曲线范围分别为11.2～112 μg·mL^-1和1.04～52 μg·mL^-1，重复性的RSD（n=6）分别为3.7%和1.7%，3种浓度的平均回收率分别为101.3%～105.4%和98.8%～101.0%，日间精密度的RSD（n=9）分别为2.7%和1.7%。9批样品中3批检出苯巴比妥，1批检出苯巴比妥和卡马西平。结论：本方法专属性强，操作简单，快捷，可作为中成药中非法添加苯巴比妥和卡马西平的有效检测方法。

Objective: To develop a UPLC-MS/MS method to determine the phenobarbital and carbamazepine illegally added in traditional Chinese anti-epileptic drugs. Methods: The analysis was performed by a UPLC-MS/MS system of Waters ACQUITY UPLC/Quattro Premier,using the BEH-C₁₈ column(100 mm×2.1 mm,1.7 μm) for separation and 0.02 mol·L^-1 ammonium acetate-acetonitrile(1: 1) as the mobile phase.Multiple-reaction monitoring(MRM) was performed to identify and quantify phenobarbital and carbamazepine which were extracted with methanol by ultrasonic. Results: The retention time was 1.1 min for phenobarbital and 1.3 min for carbamazepine.The limits of detection(LOD) for the two chemicals were 2.2 μg·mL^-1 and 0.10 μg·mL^-1.The limits of quantification(LOQ) were 7.5 μg·mL^-1 and 0.35 μg·mL^-1.The linearity ranges were 11.2-112 μg·mL^-1 and 1.04-52 μg·mL^-1.The RSDs(n=6) of reproducibility were 3.7% and 1.7%.The average recoveries of three concentration levels were 101.3%-105.4% and 98.8%-101.0%.The RSDs (n=9) of inter-day precision were 2.7% and 1.7%.Three of the nine pieces of traditional Chinese anti-epileptic drugs were found to contain phenobarbital,and one of the samples contained phenobarbital and carbamazepine. Conclusion: The method is specific,simple and fast to detect phenobarbital and carbamazepine illegally added in traditional Chinese drugs.